関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Hydroxypicolinamide | HCID 70277 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | 3-(Ethoxycarbonylmethoxy)picolinamide | HCID 22038576 | 53.3% |
反応手順
A mixture of 3-hydroxy picolinic amide (10 g, 72 mmol), ethyl bromoacetate (12.02 g, 72 mmol) and anhydrous potassium carbonate (10.9 g, 79.2 mmol) in 250 ml of dry 2-butanone is heated at 80° C. for 20 hours. After cooling, the inorganic salts are filtered off and the filtrate is reduced to approximately 120 ml. After addition of cold t-butyl methyl ether the resulting precipitate is filtered off, rinsed with cold t-butyl methyl ether and dried to give 8.6 g of 3-(ethoxycarbonylmethoxy)picolinamide (53%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07253181B2 |
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| 出典データセット | uspto-grants-2007_08 |
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| ORD ID | ord-d46b9876ddc042ef82e51d9232b17005 |
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| 出典メモ | uspto-grants-2007_08 |
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